CN106707033B - A kind of alternating temperature dielectric constant measurement pond for liquid and solid-liquid phase change - Google Patents
A kind of alternating temperature dielectric constant measurement pond for liquid and solid-liquid phase change Download PDFInfo
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- CN106707033B CN106707033B CN201611125859.0A CN201611125859A CN106707033B CN 106707033 B CN106707033 B CN 106707033B CN 201611125859 A CN201611125859 A CN 201611125859A CN 106707033 B CN106707033 B CN 106707033B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R27/00—Arrangements for measuring resistance, reactance, impedance, or electric characteristics derived therefrom
- G01R27/02—Measuring real or complex resistance, reactance, impedance, or other two-pole characteristics derived therefrom, e.g. time constant
- G01R27/26—Measuring inductance or capacitance; Measuring quality factor, e.g. by using the resonance method; Measuring loss factor; Measuring dielectric constants ; Measuring impedance or related variables
- G01R27/2617—Measuring dielectric properties, e.g. constants
- G01R27/2623—Measuring-systems or electronic circuits
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R27/00—Arrangements for measuring resistance, reactance, impedance, or electric characteristics derived therefrom
- G01R27/02—Measuring real or complex resistance, reactance, impedance, or other two-pole characteristics derived therefrom, e.g. time constant
- G01R27/26—Measuring inductance or capacitance; Measuring quality factor, e.g. by using the resonance method; Measuring loss factor; Measuring dielectric constants ; Measuring impedance or related variables
- G01R27/2617—Measuring dielectric properties, e.g. constants
- G01R27/2635—Sample holders, electrodes or excitation arrangements, e.g. sensors or measuring cells
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Abstract
A kind of alternating temperature dielectric constant measurement pond for liquid and solid-liquid phase change comprising the components such as top electrode, lower electrode, guard electrode, upper cover, liner, shell, intake-outlet connector, thermocouple, BNC adapter.Each component can cooperate, and formation stable structure, leakproofness is good, can adjust sample temperature alternating temperature dielectric constant measurement pond in real time.A kind of alternating temperature dielectric constant measurement pond for liquid and solid-liquid phase change of the invention, it is connect with circulation constant temperature water-bath machine, impedance analyzer, it realizes accurate control to sample temperature, and can accurately measure liquid at different temperatures and change in dielectric constant when occurring solid-liquid phase change；Measuring cell stable structure, anti-vibration, electromagnetic disturbance are strong, and measured data redundancy is high；When carrying out alternating temperature to liquid and solid-liquid phase change occurring, it can guarantee that sample contacts closely with electrode, it is ensured that the confidence level of data measured；Reduce the cost and maintenance difficulties of the measurement of dielectric alternating temperature.
Description
Technical field
The present invention relates to the measurement of dielectric constant more particularly to a kind of liquid alternating temperature and liquid when solid-liquid phase change occurs
Dielectric constant measurement pond.
Background technique:
When fluid temperature changes and solid-liquid phase change occurs for liquid itself, for its dielectric constant, currently with
Impedance analyzer measures it.In conventional method, structure is carried out to measuring cell based on two electrode runs parallel plate capacitor methods
Design.Its structure is to separate power-on and power-off pole piece using quartz fibre；By measuring the capacitor of air and sample, final utilize is surveyed
The ratio between sample capacitor and air capacitor for obtaining, obtain the relative dielectric constant of sample.When adding sample, need according to sample
The characteristic of product and select measuring cell, can be by sample if sample is non-volatile within the scope of measured temperature, and non-toxic, non-corrosive
Product are directly added dropwise between two electrode slices；If there are volatility within the scope of measured temperature for sample, or have toxicity, corrosivity,
It then needs to utilize the liquid measure pond with sealing characteristics.Leakproofness liquid measure pond, is that Teflon is added between upper/lower electrode
Imperial liner, and O-ring seal is added between Teflon liner and power-on and power-off pole plate.Under the compressing of external force, between electrode slice
To form closed space, to prevent sample volatilization and leakage；It is still separated using quartz fibre between electrode slice.In order to make sample
Temperature change occurs for product, carries out temperature control to sample frequently with liquid nitrogen alternating temperature furnace and temperature control digital display circuit.But this routine side
There are following disadvantages for method:
1. when using quartz fibre isolation power-on and power-off pole piece, since the placement position of quartz fibre has randomness；And
When installing electrode slice, electrode slice is easy to drive liquid in pond, and then changes the placement position of quartz fibre.Both of which
It is easy to make to cannot keep between two electrode slices parallel.This non-parallel state increases the randomness of electrode spacing, and can not
Guarantee to be consistent before and after electrode spacing after replacing sample.The change of this electrode spacing can be to same sample in different measurements
The capacitance of obtained sample causes a deviation in number.Again since quartz fibre diameter is minimum, according toIn electrode
When spacing is minimum, the change of very little can generate strong influence to surveyed capacitor, and then lead to the dielectric constant of gained sample
There are biggish deviation and nonrepeatability.
2. solid-liquid phase change occurs for sample, since sealing liquid sample pool inner space does not reserve surplus；And liquid
When body is undergone phase transition, it often will appear the contraction or expansion of sample volume.Thus when sample volume changes, such measurement
Pond not can guarantee to have between sample and electrode slice and well contact, and then measured dielectric constant is made to generate deviation.
3. liquid nitrogen alternating temperature furnace and the temperature control digital display circuit to match, involve great expense, bulky, and need in the running
A large amount of liquid nitrogen is consumed, thus limits the popularity of sample alternating temperature measurement, improves measurement threshold and maintenance difficulties.
Summary of the invention:
The technical problem to be solved in the present invention is to provide a kind of accuracy of measurement height, strong interference immunity, good airproof performance, cost
Cheap, maintenance it is simple and can precise measurement fluid temperature change and dielectric constant when solid-liquid phase change occurs for liquid
Measuring cell.
In order to solve the above technical problems, the present invention adopts the following technical scheme:
A kind of alternating temperature dielectric constant measurement pond for liquid and solid-liquid phase change, including top electrode, lower electrode, protection electricity
The components such as pole, upper cover, liner, shell, intake-outlet connector, thermocouple, BNC adapter；Wherein top electrode, lower electrode, on
Lid, liner, the shape of shell are symmetrical for axle center.Top electrode and lower electrode are all made of disk sheet metal with metallic rod；Disk gold
Belong to piece and incidentally connect step, step is included with threaded hole；Metallic rod is attached to screw thread, can pass through the spiral shell subsidiary with disk sheet metal
Pit connection, becomes T-type electrode.Guard electrode is cylindrical shape, and is attached to connection step, axially extending bore, screw thread.Upper cover is T-type
Axle center symmetrical structure, subsidiary screw thread, axially extending bore, seal groove, slot electrode.Liner is axle center symmetrical structure, subsidiary countersunk head through-hole,
Axially extending bore, screw thread, slot electrode and seal groove.Housing profile is to remove top hollow cylindrical, subsidiary threaded hole, axially extending bore, axis
To threaded hole and radial screw bore.
Alternating temperature dielectric constant measurement pond for liquid and solid-liquid phase change of the invention, upper cover, liner, the maximum of shell are outer
Diameter is consistent；The subsidiary screw thread of the upper cover screw thread subsidiary with liner can cooperate；Upper cover bottom and inner side of liner bottom
After completing assembly, there are certain spacing；Upper cover axially extending bore can be matched with the axially extending bore of guard electrode；Protection electricity
Pole internal diameter is consistent with upper cover base diameter, and is capable of forming cooperation；Guard electrode outer diameter and lower electrode discs diameter are kept
Unanimously；Top electrode disk diameter is slightly less than guard electrode internal diameter；The subsidiary slot electrode diameter of upper cover and top electrode disk diameter are protected
It holds unanimously, and can match；The subsidiary slot electrode diameter of liner is consistent with lower electrode diameter, and can be matched；On
Lid axis through-hole diameter is consistent with top electrode screw diameter, and is able to maintain loose fit；Liner axis through-hole diameter is under
Electrode screw diameter is consistent, and is able to maintain loose fit；The straight outer diameter in liner bottom end is slightly less than outer casing through hole diameter；Liner
The countersunk head through-hole axial threaded hole subsidiary with shell matches；After completing assembly, the bottom of the two is in same for liner and shell
One plane.
Alternating temperature dielectric constant measurement pond for liquid and solid-liquid phase change of the invention, upper cover and liner are carried out by screw thread
Assembly；Liner is assembled with shell by countersunk head screw, and forms sealing using sealing ring；Upper cover, liner, shell are filling
It is coaxial core structure after matching.Top electrode is fixed on upper lid by the subsidiary screw thread of metallic rod and nut, and at electrode slice back
Match sealing ring；Lower electrode is fixed on liner by the screw thread in metallic rod with nut, and is matched at electrode slice back
Sealing ring；Guard electrode is looped around top electrode surrounding and benefit is screwed on lid, and matches sealing ring；Thermocouple passes through
Upper cover axially extending bore is close to top electrode；The radial screw bore and metal connector of shell are assembled to form entery and delivery port, water inlet position
In bottom end, water outlet is located at top.
Alternating temperature dielectric constant measurement pond for liquid and solid-liquid phase change of the invention, upper/lower electrode utilize BNC adapter
It is connect with impedance analyzer BNC signal wire；Entery and delivery port using rubber tube respectively with the feed water inlet of circulation constant temperature water-bath machine and enter
Mouth of a river connection, rubber tube are surrounded by insulating tube outside；Guard electrode and entery and delivery port ground connection.
Using the claim alternating temperature dielectric constant measurement pond for liquid and solid-liquid phase change of the invention, sample is carried out
When amount, with the following method:
(1) measuring cell inside and electrode slice are cleaned using pure water, ethyl alcohol, acetone；
(2) measuring cell is calibrated using the KCl aqueous solution of air, ethyl alcohol, pure water and various concentration, obtains measuring cell
Pond constant, the capacitor that swims, residual inductance (be detailed in " Chemical Experiment in Modern Times method and technology ", publishing house, Beijing Normal University,
2010.8,160-164 page)；
(3) fluid sample is added, alternating temperature is carried out to sample using thermostatic circulation bath machine, detects sample temperature using thermocouple
Degree, and the capacitor of sample, conductance numerical value at each temperature are measured using impedance analyzer；
(4) show that the true dielectric constant of sample and alternation conductivity (are detailed in " Chemical Experiment in Modern Times side using calibration equation
Method and technology ", publishing house, Beijing Normal University, page 2010.8,160-164)；
(5) sample is taken out, measuring cell is cleaned, measurement process is completed.
It is of the invention for the alternating temperature dielectric constant measurement pond of liquid and solid-liquid phase change compared with the existing technology the advantages of are as follows:
(1) it since upper/lower electrode is separately fixed among upper cover and liner, and is carried out between upper cover and liner using screw thread
Assembly, therefore during replacing sample repeatedly, electrode spacing will not occur significantly to change, to improve dielectric constant
The data repeatability and reliability of measurement；
(2) guard electrode effectively shields outfield interference, ensure that the accuracy of dielectric constant measurement；And it is actually answering
The alternating temperature dielectric constant measurement pond of used time, liquid of the invention and solid-liquid phase change shows very strong antivibration kinetic force, anti-electromagnetism
Interference performance, i.e., when obvious vibration, large scale electronic equipment operation occur for sample cell periphery, dielectric constant measured by sample is not
It has and significantly changes, which enhance the accuracys of dielectric constant measurement；
(3) due to providing spatial margin in liner, when because of temperature or phase transformation volume expansion occurs for liquid, Neng Gouyou
The space expanded enough；And when volume is shunk, liquid can carry out in time in the space to missing under gravity
Supplement increase the reliability and accuracy of dielectric constant measurement to ensure that well contacting for sample and electrode slice；
(4) the alternating temperature dielectric constant measurement pond of liquid of the invention and solid-liquid phase change only need with thermostatic circulation bath machine into
Row matching.Compared to liquid nitrogen alternating temperature furnace and its temperature control digital display circuit, cheap, maintenance simply, thus reduces liquid and consolidates
The threshold for the alternating temperature dielectric constant measurement that liquid phase becomes.
Detailed description of the invention:
Fig. 1 is the side view of guard electrode；
Fig. 2 is the top view of guard electrode
Fig. 3 is the side view of power-on and power-off pole piece and connecting rod；
Fig. 4 is the side view of liner
Fig. 5 is the top view of liner
Fig. 6 is the side view of upper cover
Fig. 7 is the top view of upper cover
The side view of the position Fig. 8 shell
Fig. 9 is the top view of shell
Figure 10 is main view half-sectional view of the present invention for the alternating temperature dielectric constant measurement pond of liquid and solid-liquid phase change
Specific embodiment:
1. as shown in Figure 4, Figure 5, in the seal groove 8, seal groove 11 of liner add O-ring seal, and be pressed into as
In shell shown in Fig. 8, and liner and shell are fixed by through-hole 6 and threaded hole 21 using counterbore screw, makes the interior of inclusion
Portion space forms sealing；At the water inlet 22, water outlet 23 of shell two sides, metal connector is screwed in using unsintered tape,
Make its sealing；Metal connector is connect using rubber tube with thermostatic circulation bath machine；Starting thermostatic circulation bath machine is simultaneously opened
Outer circulation makes thermostatic circulation bath machine and measuring cell form closed circulating system；Circulator bath machine outer circulation flux is adjusted, is seen
Examine whether measuring cell shell and liner junction and water inlet 22,23 junction of water outlet have water (or other alternating temperature media) stream
Out；, should be by disassembling shell if still there are flowing out, and sealing ring and unsintered tape are readjusted, and be sealed；Retest makes
Final anhydrous (or other alternating temperature media) outflow.
2. inner surface, figure after Fig. 4 liner and Fig. 8 shell assemble, using pure water, ethyl alcohol, acetone to Fig. 4 liner
6 upper covers, Fig. 3 power-on and power-off pole piece, Fig. 1 guard electrode are cleaned repeatedly；After cleaning, Fig. 6 upper cover seal groove 16 with
O-ring seal is loaded onto the seal groove 10 of Fig. 4 liner, and the upper and lower electrode of Fig. 3 is assembled by screw thread 3 and screw thread 4, then
It is inserted into slot electrode 9 and slot electrode 17 respectively by through-hole 12 and through-hole 14；In the through-hole end, matched using nut, gasket and screw thread 5
It closes, fixes upper and lower electrode slice；O-ring seal is added in the seal groove 18 of Fig. 6 upper cover, covers figure 1 above guard electrode, and benefit
It is fixed by through-hole 1 with through-hole 6 with screw, nut；The upper cover assembled is merged into rotation with the matching of screw thread 7 by screw thread 15
Enter in liner, forms the alternating temperature dielectric constant measurement pond of liquid and solid-liquid phase change of the invention.
3. re-using rubber tube and accessing thermostatic circulation bath the water inlet 22 of the measuring cell assembled and water outlet 23
Machine, rubber tube wrap insulating tube outside；Target temperature is set by thermostatic circulation bath machine, outer circulation is opened, certain stream is set
Amount makes between measuring cell Fig. 4 liner and Fig. 8 shell full of water (or other alternating temperature media)；By the screw thread 5 of the upper and lower electrode slice of Fig. 3
It is utilized respectively the BNC data line of BNC adapter access impedance analyzer；By Fig. 1 guard electrode, water inlet 22 and water outlet 23
Metal connector ground connection；By the through-hole 20 of the disalignment of Fig. 6 upper cover, thermocouple is added, checks the temperature in measuring cell.
4. the method for adding sample are as follows: screw out Fig. 6 upper cover from Fig. 4 liner, after a certain amount of sample is added, revolve again
Tightly；The additive amount of sample should be higher than that the height of Fig. 3 top electrode disk.When the temperature that the thermocouple on measuring cell is detected reaches mesh
When marking temperature, measure.
5. the capacitor and electricity of air, ethyl alcohol, pure water in sample cell when measuring 20 degrees Celsius respectively using impedance analyzer
It leads；The capacitor of air, ethyl alcohol pure water is extracted, and consults the standard dielectric constant of three；Using standard dielectric constant as horizontal seat
Mark, using the capacitor surveyed as total coordinate, and continues linear fit, and resulting slope is pond constant, and intercept is to swim
Capacitor；The KCL solution for measuring various concentration, obtains its capacitor and electric conductivity value；Using conductance square as abscissa, electricity is utilized
Hold and be used as ordinate, and carries out linear fit, the residual inductance that gained slope is negative.(it is detailed in " Chemical Experiment in Modern Times method and skill
Art ", publishing house, Beijing Normal University, page 2010.8,160-164)
6. cleaning measuring cell, and sample to be tested is added, adjusts sample temperature using thermostatic circulation bath machine, and utilize impedance
Analyzer measures the capacitor and electric conductivity value of the sample at each temperature；The actual capacitance and electricity of sample are obtained using calibration equation
It leads；The true dielectric constant and conductivity of sample are obtained using correlation formula.(it is detailed in " Chemical Experiment in Modern Times method and technology ",
Publishing house, Beijing Normal University, page 2010.8,160-164)
7. taking out sample, measuring cell is cleaned, measurement terminates.
Embodiment described above only describe the preferred embodiments of the invention, not to model of the invention
It encloses and is defined, without departing from the spirit of the design of the present invention, those of ordinary skill in the art are to technical side of the invention
The various changes and improvements that case is made should all be fallen into the protection scope that claims of the present invention determines.
Claims (2)
1. a kind of alternating temperature dielectric constant measurement pond for liquid and solid-liquid phase change, it is characterised in that: including top electrode, lower electricity
Pole, guard electrode, upper cover, liner, shell, intake-outlet connector, thermocouple, BNC adapter；Wherein top electrode, lower electrode,
Upper cover, liner, the shape of shell are symmetrical for axle center；Top electrode and lower electrode are all made of disk sheet metal with metallic rod；Disk
Sheet metal incidentally connects step, and step is included with threaded hole；Metallic rod is attached to screw thread, screw thread that can be subsidiary with disk sheet metal
Hole connection, becomes T-type electrode；Guard electrode is cylindrical shape, and is attached to connection step, axially extending bore, screw thread；Upper cover is T-type axis
Heart symmetrical structure, subsidiary screw thread, axially extending bore, seal groove, slot electrode；Liner is axle center symmetrical structure, subsidiary countersunk head through-hole, axis
To through-hole, screw thread, slot electrode and seal groove；Housing profile is to remove top hollow cylindrical, subsidiary threaded hole, axially extending bore, axial direction
Threaded hole and radial screw bore；
Wherein, upper cover, liner, shell maximum outside diameter be consistent；The subsidiary screw thread of upper cover and the subsidiary screw thread of liner can
It cooperates；Upper cover bottom and inner side of liner bottom are after completing assembly, and there are certain spacing；Upper cover axially extending bore and protection
The axially extending bore of electrode can match；Guard electrode internal diameter is consistent with upper cover base diameter, and is capable of forming cooperation；It protects
Shield electrode outer diameter is consistent with lower electrode discs diameter；Top electrode disk diameter is slightly less than guard electrode internal diameter；Upper cover is subsidiary
Slot electrode diameter be consistent with top electrode disk diameter, and can match；The subsidiary slot electrode diameter of liner and lower electricity
Polar diameter is consistent, and can be matched；Upper cover axis through-hole diameter is consistent with top electrode screw diameter, and can be protected
Hold loose fit；Liner axis through-hole diameter is consistent with lower electrode screw diameter, and is able to maintain loose fit；Liner bottom end is straight
Outer diameter is slightly less than outer casing through hole diameter；The axial threaded hole that the countersunk head through-hole of liner is subsidiary with shell matches；Liner and shell
After completing assembly, the bottom of the two is in same plane；
Upper cover is assembled with liner by screw thread；Liner is assembled with shell by countersunk head screw, and utilizes sealing ring shape
At sealing；Upper cover, liner, shell are coaxial core structure after mounting；The top electrode screw thread and nut subsidiary by metallic rod
It is fixed on lid, and matches sealing ring at electrode slice back；Lower electrode is fixed on by the screw thread in metallic rod with nut interior
On gallbladder, and sealing ring is matched at electrode slice back；Guard electrode is looped around top electrode surrounding and benefit is screwed on lid,
And match sealing ring；Thermocouple is by upper cover axially extending bore close to top electrode；The radial screw bore and metal connector of shell fill
With entery and delivery port is formed, water inlet is located at bottom end, and water outlet is located at top；
Upper/lower electrode is connect using BNC adapter with impedance analyzer BNC signal wire；Entery and delivery port using rubber tube respectively with
The feed water inlet of circulation constant temperature water-bath machine is connected with water inlet, and insulating tube is surrounded by outside rubber tube；Guard electrode and entery and delivery port connect
Ground.
2. using it is described in claim 1 for the alternating temperature dielectric constant measurement pond of liquid and solid-liquid phase change measurement liquid alternating temperature and
The method of dielectric constant when generation solid-liquid phase change, it is characterised in that:
(1) measuring cell inside and electrode slice are cleaned using pure water, ethyl alcohol, acetone；
(2) measuring cell is calibrated using the KCl aqueous solution of air, ethyl alcohol, pure water and various concentration, obtains the pond of measuring cell
Constant, the capacitor that swims, residual inductance；
(3) fluid sample is added, alternating temperature is carried out to sample using thermostatic circulation bath machine, detects sample temperature using thermocouple,
And the capacitor of sample, conductance numerical value at each temperature are measured using impedance analyzer；
(4) the true dielectric constant and alternation conductivity of sample are obtained using calibration equation；
(5) sample is taken out, measuring cell is cleaned, measurement process is completed.
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| CN108195882A (en) * | 2018-02-24 | 2018-06-22 | 青岛允天保温科技有限公司 | A kind of phase transition process monitoring device and its monitoring system |
| CN110749622B (en) * | 2019-09-23 | 2022-04-26 | 杭州电子科技大学 | Solution uniformity detection device and method based on adjustable discontinuous parallel electrode plates |
| CN111157587B (en) * | 2019-12-30 | 2021-02-23 | 中国人民解放军军事科学院国防科技创新研究院 | Conductivity sensor for microgravity environment |
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